CN110423248A - A kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride - Google Patents
A kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride Download PDFInfo
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- CN110423248A CN110423248A CN201910733350.1A CN201910733350A CN110423248A CN 110423248 A CN110423248 A CN 110423248A CN 201910733350 A CN201910733350 A CN 201910733350A CN 110423248 A CN110423248 A CN 110423248A
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- tin
- monobutyl
- trichloride
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- coating liquid
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- YMLFYGFCXGNERH-UHFFFAOYSA-K butyltin trichloride Chemical compound CCCC[Sn](Cl)(Cl)Cl YMLFYGFCXGNERH-UHFFFAOYSA-K 0.000 title claims abstract description 37
- 239000011521 glass Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000007788 liquid Substances 0.000 title claims abstract description 19
- 239000011248 coating agent Substances 0.000 title claims abstract description 16
- 238000000576 coating method Methods 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 23
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- AFCAKJKUYFLYFK-UHFFFAOYSA-N tetrabutyltin Chemical compound CCCC[Sn](CCCC)(CCCC)CCCC AFCAKJKUYFLYFK-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 15
- 239000010959 steel Substances 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 10
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010792 warming Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000009413 insulation Methods 0.000 claims abstract description 6
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 6
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical class CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000007664 blowing Methods 0.000 claims abstract description 4
- 238000004821 distillation Methods 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 abstract description 11
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- RJGHQTVXGKYATR-UHFFFAOYSA-L dibutyl(dichloro)stannane Chemical compound CCCC[Sn](Cl)(Cl)CCCC RJGHQTVXGKYATR-UHFFFAOYSA-L 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- GCTFWCDSFPMHHS-UHFFFAOYSA-M Tributyltin chloride Chemical compound CCCC[Sn](Cl)(CCCC)CCCC GCTFWCDSFPMHHS-UHFFFAOYSA-M 0.000 description 5
- 239000012043 crude product Substances 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- NPAIMXWXWPJRES-UHFFFAOYSA-N butyltin(3+) Chemical compound CCCC[Sn+3] NPAIMXWXWPJRES-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- QOOQLKSEGVNYLA-UHFFFAOYSA-N 1-$l^{1}-oxidanylbutane Chemical compound CCCC[O] QOOQLKSEGVNYLA-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- REOJLIXKJWXUGB-UHFFFAOYSA-N mofebutazone Chemical group O=C1C(CCCC)C(=O)NN1C1=CC=CC=C1 REOJLIXKJWXUGB-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- YSCVYRUCAPMZFG-UHFFFAOYSA-K trichlorotin Chemical compound Cl[Sn](Cl)Cl YSCVYRUCAPMZFG-UHFFFAOYSA-K 0.000 description 2
- GGAUUQHSCNMCAU-ZXZARUISSA-N (2s,3r)-butane-1,2,3,4-tetracarboxylic acid Chemical compound OC(=O)C[C@H](C(O)=O)[C@H](C(O)=O)CC(O)=O GGAUUQHSCNMCAU-ZXZARUISSA-N 0.000 description 1
- JKIZIKMXKUMCJT-UHFFFAOYSA-K C(CCC)[Sn](CCCC)(CCCC)CCCC.C(CCC)[Sn](Cl)(Cl)Cl Chemical compound C(CCC)[Sn](CCCC)(CCCC)CCCC.C(CCC)[Sn](Cl)(Cl)Cl JKIZIKMXKUMCJT-UHFFFAOYSA-K 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ZCILODAAHLISPY-UHFFFAOYSA-N biphenyl ether Natural products C1=C(CC=C)C(O)=CC(OC=2C(=CC(CC=C)=CC=2)O)=C1 ZCILODAAHLISPY-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/22—Tin compounds
- C07F7/2208—Compounds having tin linked only to carbon, hydrogen and/or halogen
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/22—Tin compounds
- C07F7/2296—Purification, stabilisation, isolation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses a kind of preparation methods of high purity glass hot-end coating liquid monobutyl-tin-trichloride, it is related to the preparation related fields of monobutyl-tin-trichloride, the monobutyl-tin-trichloride product of high income, purity is high is obtained by the first set reaction and the subsequent processing to generation product of tin tetrachloride and tetrabutyltin, and preparation process is simple, can be carried out large-scale production.S1: tin tetrachloride is added in glassed steel reaction vessels；S2: quantitative tetrabutyltin solution being added into glassed steel reaction vessels, and insulation reaction four hours after being warming up to 100 degree；S3: quantitative water is added several times into reaction product made from S2 and is stirred layering；S4: solvent and butyl ether extraction and separation is added in water layer；S5: it weighs oil reservoir heating vacuum distillation separation, blowing after extraction to obtain monobutyl-tin-trichloride sterling.
Description
Technical field
The present invention relates to the preparation related fields of monobutyl-tin-trichloride, specially a kind of high purity glass hot-end coating liquid
The preparation method of monobutyl-tin-trichloride.
Background technique
Monobutyl-tin-trichloride (Butyltin trichloride) is abbreviated as MBTC, molecular formula C4H9Cl3Sn, molecule
Amount is 282.1833, and appearance is colorless clear transparency liquid or light yellow clear liquid, and boiling point is 93 DEG C (10mmHg), refractive index
For 1.5215-1.5245, flash-point is -10 DEG C, and boiling point is 226.8 DEG C of at 760mmHg, is dissolved in water and most of organic solvents.
It is commonly used for glass container and the spraying of specific glass surface and is sprayed in beer bottle surface, increases its hardness, it is more smooth.
Existing patent [CN 109824716A] discloses a kind of recoverying and utilizing method of tributyltin chloride, including as follows
Step: (1) tributyltin chloride by weight content less than 80% carries out high vacuum heating distillation in chlorination hydrogen atmosphere；Vacuum
Degree is 20Pa, and final warming temperature is 140 DEG C -160 DEG C；(2) by the tributyltin chloride product obtained after vacuum distillation and four
Stannic chloride mixed-controlled reaction thermotonus obtains the mixture of monobutyl-tin-trichloride and dibutyl tin dichloride；It (3) will step
Suddenly the mixture of (2) obtain monobutyl-tin-trichloride and dibutyl tin dichloride carries out distillation separation, respectively obtains monobutyl
Tin trichloride and dibutyl tin dichloride.Advantages of the present invention: final product monobutyl-tin-trichloride and dibutyl tin dichloride
Different melting points can be easily separated greatly, produces and gives up less, easy to produce, and monobutyl-tin-trichloride and dibutyl tin dichloride can be used as individually
Product use, discarded tributyltin chloride catalyst is adequately recycled, but due to this kind of method
Mainly to the recycling of tributyltin chloride, therefore the yield of independent monobutyl-tin-trichloride is not high, purity 98%, no
Enough height, cannot achieve the purpose that large-scale production.
Existing patent [CN 106977539A] provides a kind of preparation method of Mono-n-butyltin, comprising the following steps:
(1) tetrabutyltin is added into reactor, after mixing evenly, tin tetrachloride is slowly added dropwise, after being added dropwise, stirs 30min, rises
For temperature to 140 DEG C, insulation reaction 4-8h obtains the mixed solution of monobutyl-tin-trichloride, dibutyl tin dichloride；(2) by monobutyl
The mixed solution of tin trichloride, dibutyl tin dichloride is warming up to 95-100 DEG C, collects monobutyl-tin-trichloride；(3) Xiang Fanying
The monobutyl-tin-trichloride collected in step (2) is added in device, surfactant, organic solvent are slowly added dropwise after mixing evenly
Sodium hydroxide solution after being added dropwise, is warming up to 90 DEG C, and insulation reaction 3.5-4h is cooled to room temperature, and filtering obtains monobutyl oxygen
The crude product for changing tin, is washed with water the crude product of Mono-n-butyltin to neutrality, 80 DEG C are dried under reduced pressure 12h, obtain Mono-n-butyltin；By
In monobutyl-tin-trichloride as intermediate product, during the preparation process by the way that monobutyl oxygen is finally made in conjunction with other reactants
Change tin, therefore monobutyl-tin-trichloride does not have subsequent processes in pilot process, purity and yield are obviously low.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride,
The list of high income, purity is high is obtained by the first set reaction and the subsequent processing to generation product of tin tetrachloride and tetrabutyltin
Butyl tin trichloride product, and preparation process is simple, can be carried out large-scale production.
To achieve the above object, the invention provides the following technical scheme: a kind of high purity glass hot-end coating liquid monobutyl
The preparation method of tin trichloride, includes the following steps:
S1: tin tetrachloride is added in glassed steel reaction vessels；
S2: quantitative tetrabutyltin solution being added into glassed steel reaction vessels, and insulation reaction four is small after being warming up to 100 degree
When；
S3: quantitative water is added several times into reaction product made from S2 and is stirred layering；
S4: solvent and butyl ether extraction and separation is added in water layer；
S5: it weighs oil reservoir heating vacuum distillation separation, blowing after extraction to obtain monobutyl-tin-trichloride sterling.
Preferably, the tetrabutyltin and tin tetrachloride molar ratio 1:1.5-1.52.
Preferably, the tetrabutyltin and tin tetrachloride molar ratio 1:1.5.
Preferably, the range of reaction temperature of the tetrabutyltin and tin tetrachloride is 100 DEG C -120 DEG C.
Preferably, in the S2, heating mode is steam heating.
Preferably, in the S2, heating mode is electric heating.
Preferably, in the S5, distillation vacuum degree is 30mmHg.
Compared with prior art, the beneficial effects of the present invention are:
1, in the invention, tin tetrachloride and the product after tetrabutyltin are different according to density and stratification phenomenon occur,
Monobutyl-tin-trichloride crude product has been obtained at this time, then solvent and butyl ether extraction and separation will be added in water layer, by oil reservoir liter after extraction
Warm vacuum distillation separation is to obtain the monobutyl-tin-trichloride finished product of purity is high, and such purification mode is high-efficient, finally
High income, the purity is high of monobutyl-tin-trichloride finished product can be used as glass surface enhancing hot-end coating liquid and use, and whole process
In reaction it is simple, be able to carry out large-scale production；
2, use glassed steel reaction vessels as reaction vessel in the invention, because glassed steel reaction vessels are will to contain high silicon dioxide
Glass, serve as a contrast steel vessel inner surface, through high temperature sintering securely adherence on metal surface become composite material system
Product, so the two-fold advantage of stability and metal strength with glass, is a kind of excellent corrosion resistant apparatus, because in the present invention
Anhydrous stannic chloride have certain corrosivity, and tetrabutyltin is toxic, has irritation, sensitization is harmful to environment, therefore
Glassed steel reaction vessels are selected, it is corrosion-resistant, use can be reacted for a long time, and economy is strong.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.
A kind of a kind of embodiment provided by the invention: preparation side of high purity glass hot-end coating liquid monobutyl-tin-trichloride
Method includes the following steps:
S1: tin tetrachloride is added in glassed steel reaction vessels；
The corrosivity of tin tetrachloride does not have an impact to glassed steel reaction vessels, and airtightness is good, even if carrying out four fourths for a long time
Ji Xi is reacted with tin tetrachloride, will not be damaged easily；
S2: quantitative tetrabutyltin solution being added into glassed steel reaction vessels, and insulation reaction four is small after being warming up to 100 degree
When, the sufficient reaction time is given, guarantees sufficiently reaction, keeps end product amount and aim parameter error small, and tetrabutyltin and four
The range of reaction temperature of stannic chloride is 100 DEG C -120 DEG C, so needing to be warming up to 100 degree reaction can just be normally carried out；
S3: being added quantitative water into reaction product made from S2 several times and be stirred layering, according to density difference point
Layer, the small floating of density, the big sinking of density；
S4: solvent is added in water layer and butyl ether extraction and separation, butyl ether are atent solvents, the solubility (20 DEG C) to water is
0.03% (weight), water are 0.19% (weight) to (20 DEG C) of solubility of butyl ether, and the separation property with water is good, toxicity and risk
It is small, it is the very high solvent of safety, so carrying out water-oil separation as extractant using butyl ether；
S5: by oil reservoir heating vacuum distillation separation after extraction, guarantee being sufficiently separated to improve sterling for moisture and oil
Purity reduces water content therein, and blowing weighs to obtain monobutyl-tin-trichloride sterling, and yield reaches 98%, and purity reaches
99%, it can be used as glass surface enhancing hot-end coating liquid and use.
Further, tetrabutyltin and tin tetrachloride molar ratio 1:1.5-1.52, tin tetrachloride can absorb water to decompose and generate
By-product, but during the reaction, there is moisture to be decomposed in tetrabutyltin, therefore retain certain remaining reaction amount, makes four fourths
Ji Xi and tin tetrachloride can carry out normal reaction with the molar ratio of 1:1.5.
Further, tetrabutyltin and tin tetrachloride molar ratio 1:1.5.
Reaction molecular formula is 2 (C4H9)4Sn+3SnCl4→2C4H9SnCl3+3(C4H9)2SnCl2；
Product is monobutyl-tin-trichloride crude product and dibutyl tin dichloride crude product, and the density of dibutyl tin dichloride is
1.4kg/m3。
Further, in S2, heating mode is steam heating, is 100 DEG C -120 DEG C because requiring range of reaction temperature, therefore adopt
It is heated with saturated vapor, the heating upper limit of saturated vapor heating is 180 DEG C, for this reaction enough.
Further, in S2, heating mode is electric heating, and the insulating layer of glassed steel reaction vessels cylinder is wrapped in by resistance wire
On be electrically heated.
There are also water to heat for the heating method of glassed steel reaction vessels, mineral oil heating, Biphenyl Ether intermixture heats, fused salt adds
The modes such as heat, liquid lead heating, but its higher operating costs, and tetrabutyltin and tetrachloro in heating temperature section and the present invention
The reaction temperature for changing tin has difference, therefore selects steam heating or electric heating, and use cost is low, and temperature range is suitable.
Further, in S5, distillation vacuum degree is 30mmHg.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
Claims (7)
1. a kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride, which is characterized in that including walking as follows
It is rapid:
S1: tin tetrachloride is added in glassed steel reaction vessels；
S2: quantitative tetrabutyltin solution being added into glassed steel reaction vessels, and insulation reaction four hours after being warming up to 100 degree；
S3: quantitative water is added several times into reaction product made from S2 and is stirred layering；
S4: solvent and butyl ether extraction and separation is added in water layer；
S5: it weighs oil reservoir heating vacuum distillation separation, blowing after extraction to obtain monobutyl-tin-trichloride sterling.
2. a kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride according to claim 1,
It is characterized in that: the tetrabutyltin and tin tetrachloride molar ratio 1:1.5-1.52.
3. a kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride according to claim 2,
It is characterized in that: the tetrabutyltin and tin tetrachloride molar ratio 1:1.5.
4. a kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride according to claim 1,
Be characterized in that: the range of reaction temperature of the tetrabutyltin and tin tetrachloride is 100 DEG C -120 DEG C.
5. a kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride according to claim 1,
Be characterized in that: in the S2, heating mode is steam heating.
6. a kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride according to claim 1,
Be characterized in that: in the S2, heating mode is electric heating.
7. a kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride according to claim 1,
Be characterized in that: in the S5, distillation vacuum degree is 30mmHg.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910733350.1A CN110423248A (en) | 2019-08-09 | 2019-08-09 | A kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910733350.1A CN110423248A (en) | 2019-08-09 | 2019-08-09 | A kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride |
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| CN110423248A true CN110423248A (en) | 2019-11-08 |
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|---|---|---|---|
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB739883A (en) * | 1953-06-10 | 1955-11-02 | Metal & Thermit Corp | Improvements relating to the production of alkyl tin chlorides |
| US3251871A (en) * | 1961-11-15 | 1966-05-17 | Hoechst Ag | Process for the isolation of pure, watersoluble alkyl tin trihalides |
| CN102099364A (en) * | 2008-05-15 | 2011-06-15 | 阿克马法国公司 | High purity monoalkyltin compounds and uses thereof |
| CN106977539A (en) * | 2017-05-22 | 2017-07-25 | 南通艾德旺化工有限公司 | A kind of preparation method of Mono-n-butyltin |
| US20170334935A1 (en) * | 2014-12-23 | 2017-11-23 | Chemtura Corporation | Process for purifying monooctylin trichloride |
| CN109824716A (en) * | 2019-03-13 | 2019-05-31 | 南通濠泰化工产品有限公司 | A kind of recoverying and utilizing method of tributyltin chloride |
-
2019
- 2019-08-09 CN CN201910733350.1A patent/CN110423248A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB739883A (en) * | 1953-06-10 | 1955-11-02 | Metal & Thermit Corp | Improvements relating to the production of alkyl tin chlorides |
| US3251871A (en) * | 1961-11-15 | 1966-05-17 | Hoechst Ag | Process for the isolation of pure, watersoluble alkyl tin trihalides |
| CN102099364A (en) * | 2008-05-15 | 2011-06-15 | 阿克马法国公司 | High purity monoalkyltin compounds and uses thereof |
| US20170334935A1 (en) * | 2014-12-23 | 2017-11-23 | Chemtura Corporation | Process for purifying monooctylin trichloride |
| CN106977539A (en) * | 2017-05-22 | 2017-07-25 | 南通艾德旺化工有限公司 | A kind of preparation method of Mono-n-butyltin |
| CN109824716A (en) * | 2019-03-13 | 2019-05-31 | 南通濠泰化工产品有限公司 | A kind of recoverying and utilizing method of tributyltin chloride |
Non-Patent Citations (2)
| Title |
|---|
| 《化工百科全书》编辑委员会: "锡化合物", 《化工百科全书 第17卷 无机聚合物-心血管疾病药物》 * |
| 郭玉申: "单烷基有机锡化合物的性质、合成及应用", 《化学试剂》 * |
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